CN108864774A - A kind of preparation method of the reactive self-dispersing nano carbon black of cotton fabric dyeing process - Google Patents
A kind of preparation method of the reactive self-dispersing nano carbon black of cotton fabric dyeing process Download PDFInfo
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- CN108864774A CN108864774A CN201810804301.8A CN201810804301A CN108864774A CN 108864774 A CN108864774 A CN 108864774A CN 201810804301 A CN201810804301 A CN 201810804301A CN 108864774 A CN108864774 A CN 108864774A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/44—Carbon
- C09C1/48—Carbon black
- C09C1/56—Treatment of carbon black ; Purification
- C09C1/565—Treatment of carbon black ; Purification comprising an oxidative treatment with oxygen, ozone or oxygenated compounds, e.g. when such treatment occurs in a region of the furnace next to the carbon black generating reaction zone
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/10—Treatment with macromolecular organic compounds
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/58—Material containing hydroxyl groups
- D06P3/60—Natural or regenerated cellulose
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/22—Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability
Abstract
The invention discloses a kind of cotton fabric dyeing process preparation methods of reactive self-dispersing nano carbon black, belong to technical field of fine.The present invention has the group for causing polymerization of vinyl monomer function in oxidized black surface grafting functional form coupling agent first to introduce, then it selects respectively containing hydrophilic radical and can be reaction monomers with the vinyl monomer of the active group of fibrin reaction, be copolymerized using the method for in-situ polymerization and coupling agent modified carbon black.Thus, it is possible to successfully prepare the nano carbon black with reactive self-dispersing function, the hydrophilic radical on surface can guarantee that it has good self-dispersing energy in water phase；In addition, reactive group can be reacted with the hydroxyl on cotton fiber surface, to realize that chemical bonding occurs for carbon black and cotton fiber to reach the requirement of carbon black fixation.
Description
Technical field
The present invention relates to a kind of cotton fabric dyeing process preparation methods of reactive self-dispersing nano carbon black, belong to fine chemistry industry
Technical field.
Background technique
Currently, generally being dyed to cotton using black and active dye to obtain black cotton fabric of good performance.But
It is that black dyes is compounding mostly in reactive dye, since substantivity and water solubility of the dyestuff for colorant match to fiber have
Biggish difference, lead to easily to occur in dyeing course color spot and cause dyeing defect.And also need consumption a large amount of in dyeing course
Salt and bases, have a certain impact to environment.Pigment dyeing technology is early sent out in USA and Europe etc. since the middle of last century
Up to starting to apply in country, which is passed through by adding the substances such as adhesive, crosslinking agent and bleeding agent in pigment dispersion
Padding makes it be coated uniformly on fabric surface, then by preliminary drying, bake processing after, pigment anchors at fabric surface to realizing
Coloring.With conventional dyes dyeing compared with, pigment dyeing have simple process, chromatography is complete, low energy consumption, pollution less and fiber be applicable in
The features such as property is wide, therefore be increasingly valued by people.Carbon black has excellent color as a kind of important colorant
Can, it is the major colorants of black in pigment dyeing.But due in traditional coating dyes between carbon black particle and fiber only according to
Anchor at fiber surface by the embedding effect of the packet of polymer film, leading to colored fabric, often drapability is poor, Boardy Feeling, and if at
Membrane substance selection is improper, easily causes fabric in friction or water-washing process, polymer film swelling or damaged, so that fabric is resistance to
Colorfastness to rubbing and washing color fastness are poor, are significant in dye deep-colour fabric Shangyou County.In recent years, using carbon black dispersion to knitting
Object dip dyeing has also obtained the extensive concern of people, after Li carries out oxidation processes to carbon black using nitric acid, obtains that there is height to divide certainly
Scattered carbon black, and the fabrics such as cotton, acrylic fibers, wool are dyed respectively using the material.Yan Kelu etc. utilizes superfine carbon black point
Granular media dyes dacron using high temperature and high pressure method.Studies have shown that since carbon black does not have affinity to cotton fiber,
It is difficult directly upper dye fiber, fiber surface is primarily present in dyeing course, so that dyeability is very poor.Disclosed before special
The nano carbon black with self-dispersing function is successfully prepared in sharp CN106634059A, CN106634060A, but due to charcoal
It is black to lack binding force between fiber, cause the fastness of dyed fabric undesirable always, how to promote the combination jail of carbon black and fabric
Degree, becomes carbon black modified main direction of studying.
Currently, improving carbon black is mainly the following method to cotton fabric color fixation fastness：(1) cotton fabric is cation-modified.
Contain more anionic dispersing agent in carbon black dispersion, cause carbon blacksurface negatively charged, when dyeing due to fiber band
There are identical charges to cause dye-uptake lower.To improve carbon black to the dye-uptake of fiber, fiber surface can be carried out at cation
Reason, such anion carbon black particle rests against electrostatic attraction effect and is adsorbed on fiber surface, to contaminate on realizing.On but
It states and the method dyed again is first modified to fabric, process flow is longer, resource consumption is big and " dyeing flower " phenomenon can occur in dyeing.
(2) adhesive fixation.That adds suitable adhesive can obtain the preferable dyed fabric of fastness, but colored fabric often hand
Feel harder, drapability is poor.(3) functional dispersing agent.Having researcher to develop one kind has reactive polymeric dispersant,
Wherein the anchorage group of polymer can firmly be adsorbed on carbon blacksurface, reduce adverse effect caused by De contamination behavior, and
Its reactive one end can be chemically bonded with the hydroxyl on cotton fiber, to realize coloring of the carbon black to cotton fabric.This
Method can be to avoid because of the drawbacks such as fabric feeling is hard caused by using a large amount of adhesives, but since dispersing agent only relies on Van der Waals
Power, hydrogen bond etc. are adsorbed on carbon blacksurface, can remove from carbon blacksurface in dyeing course, so that carbon black particle partial size becomes in system
Greatly, so that color characteristics and level-dyeing property against color cotton fabric produce bigger effect.
For existing raising carbon black to the deficiency of cotton fabric color fixation fastness technology, the present invention attempts to contain in carbon blacksurface grafting
There is the copolymer of hydrophily and reactive functional groups.It so can be to avoid conventional carbon black dispersion because stablizing caused by De contamination
Property it is insufficient, and the coloring to realize carbon black to cotton fabric can be reacted with cotton fiber by the mode of chemical bonding.Due to this mistake
Any adhesive is not added in journey, obtained cotton fabric drapability is good, and feel is soft, and by the mode of chemical bonding, can obtain
Preferable dyefastness.
Summary of the invention
The present invention causes polymerization of vinyl monomer in oxidized black surface grafting functional form coupling agent first to introduce to have
Then the group of function selects the polymerized monomer containing hydrophilic radical and containing the polymerizable monomer with fibrin reaction group
For reaction monomers, it is copolymerized using the method for in-situ polymerization and coupling agent modified carbon black.Thus, it is possible to which successfully preparing has reactivity
The nano carbon black of self-dispersing function, the hydrophilic radical on surface can guarantee that it has good self-dispersing in water phase
Energy；In addition, reactive group can be reacted with the hydroxyl on cotton fiber surface, to realize that carbon black is chemically bonded with cotton fiber
To reach the requirement of carbon black fixation.
It is an object of the invention to develop in water phase with fine dispersion stability nano carbon black, and can by with
Hydroxyl reaction on cotton fabric, realizes that carbon black occurs covalent bond keyed with cotton fabric and colours.This method can effectively overcome tradition
The defect of poor color fastness when carbon black dispersion contaminates cotton；Meanwhile reducing the use of adhesive, it can obtain that drapability is good, feel
Soft and saturate black cotton fabric.
The first purpose of the invention is to provide a kind of reactive self-dispersing nano carbon blacks of cotton fabric dyeing process.Described is anti-
The preparation of answering property self-dispersing nano carbon black includes：Oxidation modification is carried out to carbon blacksurface, obtains oxidized black；Then in oxidation charcoal
Black surface grafting functional form coupling agent has the group for causing polymerization of vinyl monomer function to introduce, and reselection contains hydrophily
The polymerized monomer of group and containing with the polymerized monomer of fibrin reaction group be reaction monomers, with coupling agent modified carbon black be copolymerized
Come what is obtained.
In one embodiment of the invention, the carbon black is that furnace black, channel black, cracking are one of black.
In one embodiment of the invention, the oxidation modification is to carry out oxygen to carbon blacksurface using Oxygen in Liquid agent
Change and is modified.
In one embodiment of the invention, the Oxygen in Liquid agent is nitric acid solution, hydrogenperoxide steam generator, was saturated
Ammonium sulfate, perchloric acid, aqueous sodium hypochlorite solution, isocyanates solution or liquor potassic permanganate.
In one embodiment of the invention, the functional form coupling agent is the silane containing carbon-carbon double bond or sulfydryl
Coupling agent, titanate coupling agent, organic complex class coupling agent or aluminic acid compound.
In one embodiment of the invention, the polymerized monomer containing hydrophilic radical include vinyl alcohols,
Vinyl acids, vinyl amine, vinyl pyrrolidone class, vinyl sulfonic acid salt, vinylimidazolium chloride ammonium class.It is described containing
The polymerized monomer of reactive group is to contain epoxy group, a chlorine dihydroxy, isocyanate group, sulfydryl, Cyanuric Chloride, second in strand
The vinyl monomer of alkene sulfone, cyanuric fluoride etc..
In one embodiment of the invention, the copolymerization is the method using in-situ polymerization.
A second object of the present invention is to provide a kind of methods for preparing above-mentioned reactive self-dispersing nano carbon black.
The method is specifically：Oxidation modification is carried out to carbon black, obtains oxidized black；Oxidized black is added to coupling agent
Alcoholic solvent in, dispersed means are dispersed to nanoscale, and a certain amount of water is then added and adds the pH value of alkaline agent regulation system
To 8.5~9, entire reaction system is transferred in reaction kettle, coupling agent is obtained after 0.5~30h of reaction at 20~80 DEG C and changes
Property carbon black；Water-soluble monomer and reactive monomer are added into reaction kettle, is warming up to 50~90 DEG C, start that initiator is added dropwise and protects
After 0.5~20h of temperature reaction, by the centrifugation of entire reaction solution, washing, drying, the carbon black powder after drying is crushed, is obtained by filtration
Reactive self-dispersing nano carbon black powder.
In one embodiment of the invention, mass fraction of the oxidized black in alcoholic solvent be 0.1%~
40%.
In one embodiment of the invention, the alcoholic solvent is methanol, ethyl alcohol, propyl alcohol, butanol, isopropanol, second
Glycol, glycol monoethyl ether.
In one embodiment of the invention, the dispersion means are high speed disperser dispersions, emulsifier dispersion, are sanded
Machine dispersion or ultrasonic cell disruptor dispersion.
In one embodiment of the invention, the alkaline agent is sodium hydroxide, sodium carbonate, sodium bicarbonate, ammonium hydroxide, three second
Amine or triethanolamine.
In one embodiment of the invention, the additive amount of the alkaline agent is the 0.1~10% of alcoholic solvent volume fraction.
In one embodiment of the invention, the coupling agent is 10~150% to the mass fraction of oxidized black
In one embodiment of the invention, the dosage of water is to the 10~100% of alcoholic solvent mass fraction.
In one embodiment of the invention, the water-soluble monomer is 50~200% to the dosage of oxidized black.
In one embodiment of the invention, the reactive monomer is 10 to the molar ratio of water-soluble monomer：1~1：
10.
In one embodiment of the invention, the initiator is potassium peroxydisulfate, ammonium persulfate, sodium peroxydisulfate, idol
Nitrogen bis-isobutyronitrile, azo diisobutyl narrow hydrochloride, azo diisopropyl miaow mile beautiful jade hydrochloride or benzoyl peroxide.
In one embodiment of the invention, the additive amount of the initiator be sulfhydryl compound quality 0.5~
15%.
Third object of the present invention is to provide above-mentioned reactive self-dispersing nano carbon black answering in terms of cotton fabric dyeing process
With.The application is specifically：The reactive self-dispersing nano carbon black is dispersed in water, dispersed means are dispersed to nanometer
Grade is added sodium carbonate and cotton fabric and stirs evenly, be transferred in shaking water bath pot and dyed, just 30~60 DEG C of temperature of dye,
Dye 20~60min；Then temperature is increased to 60~90 DEG C, continues 20~60min of dyeing；Finally will coloring cotton fabric soap-
The cotton fabric of final carbon black dyeing is obtained after washing-drying.
In one embodiment of the invention, the reactive self-dispersing nano carbon black is to the mass fraction of cotton fabric
5~20%.
In one embodiment of the invention, the dye bath ratio is 1:20~1:60
In one embodiment of the invention, the dosage of the sodium carbonate is 5g/L~25g/L
In one embodiment of the invention, the soaping condition is:Soap flakes dosage 5g/L；Bath raio 1:50；It soaps temperature
90 DEG C of degree.
Beneficial effects of the present invention：The present invention has the group for causing monomer polymerization function by introducing in carbon blacksurface,
Then cause the vinyl monomer containing hydrophilic radical and reactive group in carbon blacksurface graft copolymerization, through centrifugation, washing,
Reactive self-dispersing nano carbon black is prepared in drying.The features such as method has simple production process, easy to operate, and grafting rate is high；System
Standby reactive self-dispersing nano carbon black has the nano carbon black of fine dispersion stability in water phase and can be by knitting with cotton
Hydroxyl reaction on object, to realize that it occurs covalent bond keyed with cotton fabric and colours.This method can effectively overcome traditional charcoal
The defect of poor color fastness when black dispersion dye cotton；Meanwhile reducing the use of adhesive, it can obtain that drapability is good, feel is soft
And saturate black cotton fabric.
Detailed description of the invention
Fig. 1：Dyeing front and back cotton fabric SEM photograph；(a) before dyeing, after (b) dyeing.
Specific embodiment
In order to be more clearly understood that technology contents of the invention, spy lifts following embodiment and is described in detail, and purpose is only
It is to be best understood from the protection scope that the contents of the present invention are not intended to limit the present invention.
Embodiment 1
Processing 0.5h is carried out to 0.6g carbon black at 20 DEG C with the nitric acid solution (concentration 30%) of 60g, oxidation is obtained and changes
The carbon black of property.It weighs 1g silane coupling agent KH590 to be dissolved in 90g ethanol solution, 1g oxidation modification carbon black is added, through ultrasonic wave
At nano particle, the deionized water of 10g is then added, and extremely with the pH value of ammonia water conditioning system in carbon black dispersion by cell disruptor
8.5, reaction system is transferred in reaction kettle, 12h is reacted at 60 DEG C, 1.5g methylacryoyloxyethyl front three is then added
Ammonium chloride and 1.2g methacrylic acid 3- chlorine-2-hydroxyl propyl ester, are warming up to 75 DEG C, start to be added dropwise monomer is weighed 1% initiation
Agent azodiisobutyronitrile reacts 4h.It finally by reaction solution high speed centrifugation, washs, drying crushes the carbon black powder after drying
Machine is ground, and is filtered with 200 mesh filter screens, and reactive self-dispersing nano carbon black can be obtained.
0.1g reactivity self-dispersing nano carbon black is dispersed in 30g water.After ultrasonication 30min, 1g cotton is added
The sodium carbonate of fabric and 5g/L simultaneously stir evenly, and are transferred in shaking water bath pot and are dyed, just 30 DEG C of temperature of dye, dyeing
60min；Then temperature is increased to 80 DEG C, continues to dye 30min；Finally will coloring cotton fabric soap-washing-obtained most after drying
Whole dyed cotton fabric.
Fig. 1 shows the SEM pictures of dyeing front and back cotton fabric in embodiment 1, the cotton fabric after as can be seen from the figure dyeing
Surface covers one layer of reactive self-dispersing nano carbon black material membrane, and fabric surface is more smooth, and carbon black particle distribution is also more uniform,
This is because its uniform adsorption occurs caused by chemical bonding in fabric surface and with cotton fabric.The result shows that institute of the present invention
The modified carbon black of preparation has good dyeability to cotton fabric.
Embodiment 2
Processing 2h is carried out to 4g carbon black at 60 DEG C with the hydrogenperoxide steam generator (concentration 30%) of 40g, oxidation is obtained and changes
The carbon black of property.It weighs 1.3g silane coupling agent KH570 to be dissolved in 60g ethanol solution, 8g oxidation modification carbon black is added, through ultrasound
At nano particle, the deionized water of 30g is then added in carbon black dispersion by wave cell disruptor, and with sodium hydroxide regulation system
Reaction system is transferred in reaction kettle, reacts at by 40 DEG C for 24 hours to 9 by pH value, it is rear be added 8g vinyl pyrrolidone and
3.5g methacrylic acid 3- chlorine-2-hydroxyl propyl ester, is warming up to 80 DEG C, start to be added dropwise monomer is weighed 2% initiator ammonium persulfate,
React 6h.It finally by reaction solution high speed centrifugation, washs, the carbon black powder after drying is ground with pulverizer, is used in combination by drying
The filtering of 200 mesh filter screens, can be obtained reactive self-dispersing nano carbon black.
0.02g reactivity self-dispersing nano carbon black is dispersed in 20g water.After ultrasonication 30min, 1g cotton is added
The sodium carbonate of fabric and 15g/L simultaneously stir evenly, and are transferred in shaking water bath pot and are dyed, just 40 DEG C of temperature of dye, dyeing
30min；Then temperature is increased to 85 DEG C, continues to dye 20min；Finally will coloring cotton fabric soap-washing-obtained most after drying
Whole dyed cotton fabric.
Embodiment 3：
Processing 2h is carried out to 4g carbon black at 50 DEG C with 40g perchloric acid solution, obtains the carbon black of oxidation modification.Weigh 2.5g
Silane coupling A 151 is dissolved in 50g ethanol solution, and 5g oxidation modification carbon black is added, through ultrasonic cell disruptor by carbon black
It is dispersed into nano particle, the deionized water of 25g is then added, and use the pH value of ammonia water conditioning system to 8.5, by reaction system turn
It moves on in reaction kettle, is reacted at 40 DEG C for 24 hours, it is rear that 10g sodium p styrene sulfonate and the chloro- 2- hydroxyl of 2g methacrylic acid 3- is added
Base propyl ester is warming up to 60 DEG C, start to be added dropwise monomer is weighed 5% initiator potassium persulfate, react 7h.Finally by reaction solution high speed
Centrifugation is washed, and drying grinds the carbon black powder after drying with pulverizer, and is filtered with 200 mesh filter screens, can be obtained
Reactive self-dispersing nano carbon black.
4g reactivity self-dispersing nano carbon black is dispersed in 480g water.After ultrasonication 30min, 80g cotton is added
The sodium carbonate of fabric and 5g/L simultaneously stir evenly, and are transferred in shaking water bath pot and are dyed, just contaminate temperature 60 C, dyeing
40min；Then temperature is increased to 90 DEG C, continues to dye 30min；Finally will coloring cotton fabric soap-washing-obtained most after drying
Whole dyed cotton fabric.
Reference examples 1：
Compared with Example 1, the non-oxidation processes of carbon black, other steps and parameter and embodiment 1 are consistent；Specifically：It weighs
1g silane coupling agent KH590 is dissolved in 90g ethanol solution, and the original carbon black of 1g is added, through ultrasonic cell disruptor by carbon black
It is dispersed into nano particle, the deionized water of 10g is then added, and use the pH value of ammonia water conditioning system to 8.5, by reaction system turn
It moves on in reaction kettle, 12h is reacted at 60 DEG C, 1.5g MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride and 1.2g is then added
Methacrylic acid 3- chlorine-2-hydroxyl propyl ester, is warming up to 75 DEG C, start to be added dropwise monomer is weighed 1% initiator azodiisobutyronitrile,
React 4h.It finally by reaction solution high speed centrifugation, washs, the carbon black powder after drying is ground with pulverizer, is used in combination by drying
The filtering of 200 mesh filter screens, can be obtained reactive self-dispersing nano carbon black.0.1g reactivity self-dispersing nano carbon black is dispersed in
In 30g water.After ultrasonication 30min, the sodium carbonate of 1g cotton fabric and 5g/L is added and stirs evenly, is transferred to concussion water
It is dyed in bath, just 30 DEG C of temperature of dye, dyes 60min；Then temperature is increased to 80 DEG C, continues to dye 30min；Finally will
Coloring cotton fabric soap-washing-final dyed cotton fabric is obtained after drying.
Reference examples 2
Compared with Example 1, the 1.2g methacrylic acid 3- chlorine-2-hydroxyl propyl ester (vinyl of reactive group is not added
Monomer), other steps and parameter and embodiment 1 are unanimously；Specifically：
Processing 0.5h is carried out to 0.6g carbon black at 20 DEG C with the nitric acid solution (concentration 30%) of 60g, oxidation is obtained and changes
The carbon black of property.It weighs 1g silane coupling agent KH590 to be dissolved in 90g ethanol solution, 1g oxidation modification carbon black is added, through ultrasonic wave
At nano particle, the deionized water of 10g is then added, and extremely with the pH value of ammonia water conditioning system in carbon black dispersion by cell disruptor
8.5, reaction system is transferred in reaction kettle, 12h is reacted at 60 DEG C, 1.5g methylacryoyloxyethyl front three is then added
Ammonium chloride is warming up to 75 DEG C, start to be added dropwise monomer is weighed 1% initiator azodiisobutyronitrile, react 4h.It finally will reaction
Liquid high speed centrifugation washs, and drying grinds the carbon black powder after drying with pulverizer, and is filtered with 200 mesh filter screens, i.e.,
Reactive self-dispersing nano carbon black can be obtained.0.1g reactivity self-dispersing nano carbon black is dispersed in 30g water.At ultrasonic wave
After managing 30min, the sodium carbonate of 1g cotton fabric and 5g/L is added and stirs evenly, is transferred in shaking water bath pot and is dyed, just
30 DEG C of temperature of dye dyes 60min；Then temperature is increased to 80 DEG C, continues to dye 30min；Finally coloring cotton fabric is soaped-water
Final dyed cotton fabric is obtained after washing-drying.
Reference examples 3
Compared with Example 1, it is not added with the 1.5g MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride (second in hydrophilic monomer
Alkenyl amine), other steps and parameter and embodiment 1 are unanimously；As the result is shown：Dispersion performance is very poor, is difficult to carry out to fiber
Dye.
Specifically：Processing 0.5h is carried out to 0.6g carbon black at 20 DEG C with the nitric acid solution (concentration 30%) of 60g, is obtained
The carbon black of oxidation modification.It weighs 1g silane coupling agent KH590 to be dissolved in 90g ethanol solution, 1g oxidation modification carbon black, warp is added
At nano particle, the deionized water of 10g is then added in carbon black dispersion by ultrasonic cell disruptor, and with ammonia water conditioning system
Reaction system is transferred in reaction kettle to 8.5,12h is reacted at 60 DEG C, be then added and 1.2g methacrylic acid by pH value
3- chlorine-2-hydroxyl propyl ester, is warming up to 75 DEG C, start to be added dropwise monomer is weighed 1% initiator azodiisobutyronitrile, react 4h.Most
It afterwards by reaction solution high speed centrifugation, washs, drying grinds the carbon black powder after drying with pulverizer, and with 200 mesh filter screens
Filtering, can be obtained reactive self-dispersing nano carbon black.0.1g reactivity self-dispersing nano carbon black is dispersed in 30g water.Through
After ultrasonication 30min, the sodium carbonate of 1g cotton fabric and 5g/L is added and stirs evenly, is transferred in shaking water bath pot and carries out
Dyeing, just 30 DEG C of temperature of dye, dyes 60min；Then temperature is increased to 80 DEG C, continues to dye 30min；Cotton fabric will finally be coloured
Soap-washing-final dyed cotton fabric is obtained after drying.
The stably dispersing performance and its dyeability to cotton fabric of the nano carbon black sample of 1 distinct methods of table preparation
Note：SS(storage stability)：Transparent sample bottle will be placed on by rear carbon black dispersion (solid content 10%) before modified
In, there is the time precipitated in observation bottom of bottle.ST(heat-resistant stability)：2mL carbon black dispersion liquid is taken, it is placed into 2h at 60 DEG C,
After take the upper layer 1mL dispersion liquid, be diluted to certain multiple, respectively test place carbon black dispersion liquid before and after the processing partial size it is big
It is small, its heat-resistant stability is tested according to formula 1.SC(centrifugal stability)：2mL carbon black dispersion liquid is taken, is placed it in
In Centrifuge 5415D type supercentrifuge, to be centrifugated 30min under 3000r/min speed, 1mL is taken after centrifugation
Upper layer dispersion liquid is diluted to certain multiple, and the particle size of test centrifugation front and back carbon black dispersion liquid, is tested according to formula 2 respectively
Its centrifugal stability.
Wherein, d0Indicate the partial size of carbon black dispersion liquid when untreated (do not heat or centrifugal treating), dTIndicate carbon black dispersion liquid
Partial size after placing at different temperatures, dCIndicate the partial size after carbon black dispersion liquid is centrifuged under different centrifugal speeds.
K/S (tinctorial yield of original liquid coloring fiber) by 8400 type Computer color testing of X-RITE color matching instrument use D65 light source, 10 °
It is measured under viewing angle.Difference test is taken on dyed cotton fabric three times, is averaged, and according to formula 3, calculates K/S value：
Wherein, R0It is the reflectivity of cotton fabric and dyed cotton fabric of being unstained respectively with R.
Rub resistance and fastness to washing coloring are tested referring to standard GB/T/29865-2013 and GB/T3921-2008.
Although the present invention has been described by way of example and in terms of the preferred embodiments, it is not intended to limit the invention, any to be familiar with this skill
The people of art can do various change and modification, therefore protection model of the invention without departing from the spirit and scope of the present invention
Enclosing subject to the definition of the claims.
Claims (10)
1. a kind of reactive self-dispersing nano carbon black of cotton fabric dyeing process, which is characterized in that the reactive self-dispersing nanometer
The preparation of carbon black includes：Oxidation modification is carried out to carbon blacksurface, obtains oxidized black；Then in oxidized black surface grafting function
Type coupling agent has the group for causing polymerization of vinyl monomer function to introduce, and reselection contains the polymerized monomer of hydrophilic radical
With containing being reaction monomers with the polymerized monomer of fibrin reaction group, it is copolymerized to obtain with coupling agent modified carbon black.
2. self-dispersing nano carbon black according to claim 1, which is characterized in that the oxidation modification is using liquid phase oxidation
Agent carries out oxidation modification to carbon blacksurface.
3. self-dispersing nano carbon black according to claim 1, which is characterized in that the water-soluble monomer includes vinyl alcohol
Class, vinyl acids, vinyl amine, vinyl pyrrolidone class, vinyl sulfonic acid salt, vinylimidazolium chloride ammonium class；It is described
Reactive monomer is to contain epoxy group, a chlorine dihydroxy, isocyanate group, sulfydryl, Cyanuric Chloride, vinyl sulfone(RemzaolHuo Xingranliaohuoxingjituan), trimerization in strand
The vinyl monomer of fluorine cyanogen etc..
4. a kind of method for preparing any reactive self-dispersing nano carbon black of claim 1-3, which is characterized in that described
Method is specifically：Oxidation modification is carried out to carbon black, obtains oxidized black；Oxidized black is added in the alcoholic solvent of coupling agent,
Dispersed means are dispersed to nanoscale, and a certain amount of water is then added and adds the pH value of alkaline agent regulation system to 8.5~9, will
Entire reaction system is transferred in reaction kettle, obtains coupling agent modified carbon black after reacting 0.5~30h at 20~80 DEG C；To anti-
Answer and water-soluble monomer and reactive monomer be added in kettle, be warming up to 50~90 DEG C, start to be added dropwise initiator and insulation reaction 0.5~
After 20h, by the centrifugation of entire reaction solution, washing, drying, the carbon black powder after drying is crushed, reactive self-dispersing is obtained by filtration
Nano carbon black powder.
5. according to the method described in claim 4, it is characterized in that, mass fraction of the oxidized black in alcoholic solvent is
0.1%~40%.
6. according to the method described in claim 4, it is characterized in that, the water-soluble monomer to the dosage of oxidized black be 50~
200%.
7. according to the method described in claim 4, it is characterized in that, the reactive monomer is to the molar ratio of water-soluble monomer
10：1~1：10.
8. application of any reactive self-dispersing nano carbon black of claim 1-3 in terms of cotton fabric dyeing process.
9. application according to claim 8, which is characterized in that the application is specifically：The reactive self-dispersing is received
In water, dispersed means are dispersed to nanoscale to rice carbon black dispersion, and sodium carbonate and cotton fabric is added and stirs evenly, is transferred to shake
It swings in water-bath and is dyed, just 30~60 DEG C of temperature of dye, dye 20~60min；Then temperature is increased to 60~90 DEG C, is continued
Dye 20~60min；Finally will coloring cotton fabric soap-washing-cotton fabric of final carbon black dyeing is obtained after drying.
10. application according to claim 9, which is characterized in that the reactivity self-dispersing nano carbon black is to cotton fabric
Mass fraction is 5~20%.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110204929A (en) * | 2019-07-11 | 2019-09-06 | 青岛大学 | A kind of method of hexa-member heterocycle covalent modification graphene oxide |
| CN110369733A (en) * | 2019-08-15 | 2019-10-25 | 盐城工学院 | A kind of preparation of self-dispersing silver-carbon dust and colouring method |
| CN111235923A (en) * | 2020-03-11 | 2020-06-05 | 华维新材料科技(杭州)有限公司 | Preparation and dyeing process of nano liquid black |
| CN112456467A (en) * | 2020-11-19 | 2021-03-09 | 沈阳化工研究院有限公司 | Modified carbon black applied to spinning resin coloring and preparation method thereof |
| CN114232364A (en) * | 2021-10-28 | 2022-03-25 | 盐城工学院 | Preparation of self-dispersion reactive nano carbon powder and dyeing method of cotton fabric by using self-dispersion reactive nano carbon powder |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08337737A (en) * | 1995-06-14 | 1996-12-24 | Nippon Shokubai Co Ltd | Surface modification of solid fine particle |
| CA2347093C (en) * | 1998-10-13 | 2009-04-07 | Cabot Corporation | Polymer coated carbon products and other pigments and methods of making same by aqueous media polymerizations or solvent coating methods |
| WO2010038835A1 (en) * | 2008-10-02 | 2010-04-08 | 株式会社ブリヂストン | Method for producing graft copolymer, graft copolymer obtained by the method, rubber composition containing the graft copolymer, and tire |
| CN106634059A (en) * | 2016-12-16 | 2017-05-10 | 江南大学 | Preparation method of aqueous self-dispersing nanometer carbon black |
| CN106634060A (en) * | 2016-12-16 | 2017-05-10 | 江南大学 | Preparation method of oily self-dispersing nano carbon black |
| WO2018016985A1 (en) * | 2016-07-22 | 2018-01-25 | Public Joint Stock Company "Sibur Holding" | A method for producing branched modified rubber and a rubber composition comprising branched modified rubber prepared by the method, and use thereof |
| CN108148443A (en) * | 2017-12-25 | 2018-06-12 | 江南大学 | Preparation method of aqueous self-dispersion nano organic pigment powder |
-
2018
- 2018-07-20 CN CN201810804301.8A patent/CN108864774B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08337737A (en) * | 1995-06-14 | 1996-12-24 | Nippon Shokubai Co Ltd | Surface modification of solid fine particle |
| CA2347093C (en) * | 1998-10-13 | 2009-04-07 | Cabot Corporation | Polymer coated carbon products and other pigments and methods of making same by aqueous media polymerizations or solvent coating methods |
| WO2010038835A1 (en) * | 2008-10-02 | 2010-04-08 | 株式会社ブリヂストン | Method for producing graft copolymer, graft copolymer obtained by the method, rubber composition containing the graft copolymer, and tire |
| WO2018016985A1 (en) * | 2016-07-22 | 2018-01-25 | Public Joint Stock Company "Sibur Holding" | A method for producing branched modified rubber and a rubber composition comprising branched modified rubber prepared by the method, and use thereof |
| CN106634059A (en) * | 2016-12-16 | 2017-05-10 | 江南大学 | Preparation method of aqueous self-dispersing nanometer carbon black |
| CN106634060A (en) * | 2016-12-16 | 2017-05-10 | 江南大学 | Preparation method of oily self-dispersing nano carbon black |
| CN108148443A (en) * | 2017-12-25 | 2018-06-12 | 江南大学 | Preparation method of aqueous self-dispersion nano organic pigment powder |
Non-Patent Citations (2)
| Title |
|---|
| 孙从振: ""反应性纳米炭黑的制备及其应用研究"", 《中国优秀硕士学位论文全文数据库》 * |
| 杨昕宇 等: ""自分散纳米炭黑色浆的制备和研究"", 《硅酸盐学报》 * |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110204929A (en) * | 2019-07-11 | 2019-09-06 | 青岛大学 | A kind of method of hexa-member heterocycle covalent modification graphene oxide |
| CN110204929B (en) * | 2019-07-11 | 2021-06-08 | 青岛大学 | Method for covalently modifying graphene oxide by using six-membered heterocyclic ring |
| CN110369733A (en) * | 2019-08-15 | 2019-10-25 | 盐城工学院 | A kind of preparation of self-dispersing silver-carbon dust and colouring method |
| CN110369733B (en) * | 2019-08-15 | 2022-05-27 | 盐城工学院 | Preparation and dyeing method of self-dispersing silver-carbon powder |
| CN111235923A (en) * | 2020-03-11 | 2020-06-05 | 华维新材料科技(杭州)有限公司 | Preparation and dyeing process of nano liquid black |
| CN111235923B (en) * | 2020-03-11 | 2022-03-25 | 华维新材料科技(杭州)有限公司 | Preparation and dyeing process of nano liquid black |
| CN112456467A (en) * | 2020-11-19 | 2021-03-09 | 沈阳化工研究院有限公司 | Modified carbon black applied to spinning resin coloring and preparation method thereof |
| CN114232364A (en) * | 2021-10-28 | 2022-03-25 | 盐城工学院 | Preparation of self-dispersion reactive nano carbon powder and dyeing method of cotton fabric by using self-dispersion reactive nano carbon powder |
| CN114232364B (en) * | 2021-10-28 | 2023-06-23 | 盐城工学院 | Preparation of self-dispersing reactive nano carbon powder and dyeing method of self-dispersing reactive nano carbon powder on cotton fabric |
| CN114561109A (en) * | 2022-01-29 | 2022-05-31 | 新疆德欣精细化工有限公司 | High-purity carbon black nano material based on powder pretreatment and preparation method thereof |
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